A new simple liquid chromatographic assay for gentamicin in presence of methylparaben and propylparaben

• Autorzy: Ivković, Branka , Milutinović, Ivana , Čudina, Olivera , Marković, Bojan
• Języki publikacji: EN

Abstrakty

EN

Gentamicin sulfate is a potent broad spectrum aminoglycoside antibiotic which is used against Gram-positive and Gram-negative bacteria. A simple, isocratic HPLC method for separation, identification and determination of gentamicin and parabens (methylparaben and propylparaben) was developed and validated. To our knowledge there is no report about simultaneous determination of those three analytes in pharmaceutical products. The optimum chromatographic conditions were achieved on CN column with a mobile phase consisting of 0.15% triethylamine in 10 mM KH₂PO₄ aqueous solution (final pH 3.0 adjusted with H₃PO₄) and methanol in the ratio 70:30 (v/v), providing selective quantification of analytes within 5 min. The method was successfully validated according to ICH guidelines acceptance criteria in terms of selectivity, linearity, accuracy, precision and robustness. The linearity of the method was proved in defined concentrations ranges for gentamicin (0.32–1.04 mg mL⁻¹), methylparaben (0.0072–0.0234 mg mL⁻¹) and propylparaben (0.0008–0.0026 mg mL⁻¹). Relative standard deviations calculated for all analytes in precision testing were <2% (analysis repeatability) and <3% (intermediate precision). Recovery values were between 98.87% and 101.67%. Chromatographic parameters are not significantly influenced by small variations of column temperature, pH and molarity of KH₂PO₄. Finally, the method was successfully applied for quantitative determination of gentamicin and parabens in commercially available solution for injection. Proposed HPLC method is found to be promising in terms of simplicity, analysis times and non-use of derivatization and ion-pair agents.

Słowa kluczowe

EN

gentamicin; liquid chromatography; parabens; validation

• Czasopismo: Acta Chromatographica
• Rocznik: 2023
• Tom: Vol. 35, no. 1
• Strony: 81--87
• Opis fizyczny: Bibliogr. 28 poz., tab., rys., wykr.

Twórcy

autor

Ivković, Branka

• Department of Pharmaceutical Chemistry, University of Belgrade - Faculty of Pharmacy, Vojvode Stepe 450, 11221, Belgrade, Serbia,

autor

Milutinović, Ivana

• Evrolek Pharmacija d.o.o, Pocerska bb, 15000, Sabac, Serbia

autor

Čudina, Olivera

• Department of Pharmaceutical Chemistry, University of Belgrade - Faculty of Pharmacy, Vojvode Stepe 450, 11221, Belgrade, Serbia

autor

Marković, Bojan

• Department of Pharmaceutical Chemistry, University of Belgrade - Faculty of Pharmacy, Vojvode Stepe 450, 11221, Belgrade, Serbia

Bibliografia

• 1. Lemke, T. L.; Zito, W. S.; Roche, V. F.; Williams, D. A. In Essentials of Foye’s Principles of Medicinal Chemistry, Abridgement of: Foye’s Principles of Medicinal Chemistry; Lemke, T. L.; Williams, D. A., Eds. Wolters Cluver: Philadelphia, 2017; pp 435–78.
• 2. Mingeot-Leclercq, M. P.; Glupczynski, Y.; Tulkens, P. M. Antimicrob. Agents Chemother. 1999, 43, 727–37.
• 3. The U.S. Pharmacopeia USP 34, NF 29. U.S. Pharmacopeial Convention, Rockville, 2011; p. 2959.
• 4. Posyniak, A.; Zmudzki, J.; Niedzielska, J. J. Chromatogr. A. 2001, 914, 59–66.
• 5. Turnipseed, S. B.; Clark, S. B.; Karbiwnyk, C. M.; Andersen, W. C; Miller, K. E.; Madson, M. R. J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. 2009, 877, 1487–93.
• 6. Larsen, N. E.; Marinelli, K.; Heilesen, A. M. J. Chromatogr. B Biomed. Appl. 1980, 221, 182–7.
• 7. Barends, D. M.; Zwaan, C. L.; Hullshoff, A. J. Chromatogr. 1981, 222, 316–23.
• 8. Walker, S. E.; Coates, P. E. J. Chromatogr. Biomed. Appl. 1981, 223, 131–8.
• 9. Weigand, R.; Coombes, R. J. J. Chromatogr. A. 1983, 281, 381–5.
• 10. Kubo, H.; Kinoshita, T.; Kobayashi, Y.; Tokunaga, K. J. Chromatogr. B Biomed. Appl. 1982, 227, 244–8.
• 11. Li, B.; Van Schepdael, A.; Hoogmartens, J.; Adams, E. J. Pharm. Biomed. Anal. 2011, 55, 78–84.
• 12. Manyanga, V.; Kreft, K.; Divjak, B.; Hoogmartens, J.; Adams, E. J. Chromatogr. A. 2008, 1189, 347–54.
• 13. Joseph, A.; Rustum, A. J. Chromatogr. A. 2010, 51, 521–31.
• 14. Manyanga, V.; Grishina, O.; Yun, Z.; Hoogmartens, J.; Adams, E. J. Pharm. Biomed. Anal. 2007, 45, 257–62.
• 15. Ianni, F.; Pucciarini, L.; Carotti, A.; Saluti, G.; Moretti, S.; Ferrone, V.; Sardella, R.; Galarini, R.; Natalini, B. Anal. Chim. Acta 2018, 1044, 174–80.
• 16. Yang, B.; Wang, L.; Luo, C.; Wang, X.; Sun, C. J. AOAC Int. 2017, 100, 1869–78.
• 17. Megoulas, N. C.; Koupparis, M. A. J. Pharm. Biomed. Anal. 2004, 36, 73–9.
• 18. British Pharmacopoeia, British Pharmacopoeia Commision, 2020.
• 19. The U.S. Pharmacopeia USP 43, NF 38. U.S. Pharmacopeial Convention, Rockville, 2020.
• 20. Rodriquez, M.; Cretoso, D. S.; Euterpio, M. A.; Russo, P.; Crescenzi, C. Anal. Bioanal. Chem. 2015, 407, 7691–701.
• 21. Lucha, S.; Taibon, J.; Pongratz, S.; Geletneky, C.; Huber, E.; Wintterle-Roehm, C.; Lang, R.; Grimm, S. H.; Duelffer, T.; Tarasov, K.; Zander, J.; Vogeser, M.; Kobold, U. Clin. Chim. Acta 2017, 464, 211–7.
• 22. Sun, X.; Yang, Y.; Tian, Q.; Shang, D.; Xing, J.; Zhai, Y. J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. 2018, 1093167–4173.
• 23. Brozmanova, H.; Urinovska, R.; Safarcik, K.; Vsiansky, F.; Kacirova, I.; Grundmann, M. Clin. Chim. Acta 2021; https://doi.org/10.1016/j.cca.2021.07.014.
• 24. Moreta, C.; Tena, M. T.; Kannan, K. Environ. Res. 2015, 142, 452–60.
• 25. Piao, C.; Chen, L.; Wang, Y. J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. 2014, 969, 139–48.
• 26. Larsen, N. E.; Marinelli, K.; Heilesen, A. M. J. Chromatogr. Biomed. Appl. 1980, 221, 182–9.
• 27. International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use, ICH Harmonised Tripartite Guideline, Validation of Analytical Procedures: Text and Methodology Q2(R1), 2005, ICH: Geneva.
• 28 Crowther, J.B. In Handbook of Modern Pharmaceutical Analysis; Ahuja, S.; Scypinsky, S., Eds. Academic Press: San Diego, USA, 2001; pp 415–40.

Uwagi

Opracowanie rekordu ze środków MEiN, umowa nr SONP/SP/546092/2022 w ramach programu "Społeczna odpowiedzialność nauki" - moduł: Popularyzacja nauki i promocja sportu (2022-2023).

Identyfikatory

DOI

10.1556/1326.2022.00999